Recent studies have revealed that electrochemistry at the nanometer scale is profoundly different from its conventional framework. We reported that the combination of a hydrophobic nanoporous electrode and low-charge-density metal ions resulted in a drastic acceleration in the electrodeposition reaction. In the present study, we analyzed Zn embedded in nanoporous silicon by X-ray absorption fine structure spectroscopy. As a precursor to Zn electrodeposition, Zn(II) chelate was used under different pH conditions. The spectroscopy results clearly suggest that the accumulation of Zn(II) chelate occurred at pH conditions where the Zn(II) chelate had zero charge. The accumulation resulted in the promotion of Zn electrodeposition within confined nanopores. Based on this spectroscopic investigation, we propose a model for the accelerated electrodeposition of Zn in confined nanopores.
The in situ study of the discharge process in a zinc‐based half‐cell employing a porous electrode as a structural scaffold is reported. The in situ characterization has been performed by synchrotron X‐ray absorption fine‐structure spectroscopy and, for this purpose, an inexpensive, simple and versatile electrochemical cell compatible with X‐ray experiments has been designed and described. The experimental results reported here have been employed to semi‐quantify the dissolved and undissolved zinc species during the discharge, allowing the cell feasibility to be tested and to better understand the functioning of the zinc half‐cell based on porous electrodes.
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